Negative-pressure extracting and separating system for organic pollutants in sample and separating method

A technology for organic pollutants and separation systems, applied in the field of negative pressure extraction and separation systems for organic pollutants in samples, can solve the problems of loss of target compounds, affecting analysis results, and high processing costs, reducing analysis costs, and achieving qualitative and quantitative accuracy. The effect of reducing secondary pollution

Pending Publication Date: 2018-03-06
谢家理
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The concentration process of the two concentration methods will take a lot of time and easily cause the loss of the target compound
[0008] In summary, the current pretreatment methods for semi-volatile organic compounds or non-volatile organic compounds, whether it is the purification method of the extract, the extraction method of the liquid matrix, or the extraction method of the solid matrix, the common feature of the above methods is that they need to use more There are many organic solvents, reagents and consumables, and large-scale pretreatment equipment is required to achieve the required extraction efficiency, and the pretreatment time is long, there are many intermediate steps, the unit sample processing cost is high, and the waste residue and liquid have the possibility of secondary pollution, and It is easy to introduce interference in the middle process and affect the analysis results
The concentration process of a large number of solvents is not only time-consuming, but also easily causes the loss of the target compound and leads to the failure of the experiment
In addition, these methods extract a large amount of impurities in the sample while extracting the target compound, which not only requires an additional purification process, but also the purification effect is difficult to guarantee, resulting in adverse effects of analytical result deviation and chromatographic service life reduction

Method used

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  • Negative-pressure extracting and separating system for organic pollutants in sample and separating method
  • Negative-pressure extracting and separating system for organic pollutants in sample and separating method
  • Negative-pressure extracting and separating system for organic pollutants in sample and separating method

Examples

Experimental program
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Effect test

Embodiment 1

[0039] The negative pressure extraction and separation system for organic pollutants in the sample used in this embodiment is as figure 1 As shown, it includes a sample bottle 2, a first sample transmission line 4, an absorption bottle 5, and a pump 10 connected in sequence. The sample bottle 2 is provided with a sample to be extracted, and the absorption bottle 5 is provided with a liquid adsorbent 6 inside. Specifically, the sample bottle jacket is provided with a sample heater 1, the absorption bottle jacket is provided with a first cooling device 7, and the first sample transfer pipeline 4 is wrapped with a first heating device 15; the sample heater 1 can be electrically heated Heaters or heat exchangers and other common heater structures on the market (because heaters are more common, so I won’t repeat them). The sample heater is set outside the sample bottle 2 to adjust the temperature of the sample bottle. The first heating The device 15 may be a common tubular heater str...

example 1

[0047] This example is to test the negative pressure extraction and separation method of organochlorine pesticides and chlorobenzene compounds in liquid phase (organic solvent phase, water phase) and solid phase (soil).

[0048] 1. Test of negative pressure extraction and separation method for organochlorine pesticides and chlorobenzene compounds with a concentration of 200μg / L in toluene

[0049] ⑴ Standard solution preparation

[0050] Prepare a liquid standard mixture of organochlorine pesticides and chlorobenzene into a mixed standard of toluene with a concentration of 100μg / mL, and then take 10mL of toluene solvent into 22mL sample bottle as a blank sample for the whole process; take 10mL of toluene solvent into 22mL sample bottle As a sample absorption bottle; take 10mL toluene solvent into a 22mL sample bottle, and add 20μL mixed standard as the measurement sample, the concentration is 200μg / L; take 20μL mixed standard into 1mL toluene as the measurement standard, the concentr...

example 2

[0094] Test of negative pressure extraction and separation method for PCBs in liquid phase (organic solvent phase, water phase) and solid phase (soil)

[0095] 1. Test method for negative pressure extraction and separation of PCBs with a concentration of 100μg / L in toluene

[0096] (1) Standard solution preparation

[0097] The liquid standard of PCBs was prepared into a toluene phase standard solution with a concentration of 10.0μg / mL.

[0098] Take 10mL of toluene solvent into a 22mL sample bottle as a blank sample throughout the process;

[0099] Take 10mL of toluene solvent into a 22mL sample bottle as a sample absorption bottle;

[0100] Take 10mL of toluene solvent into a 22mL sample bottle, and add 100μL of standard solution as the measurement sample, with a concentration of 100.0μg / L;

[0101] Take 100 μL of the standard solution into 1 mL of toluene as the determination standard, and the concentration is 1 μg / mL.

[0102] (2) Air connection

[0103] The sample heater, the sealed sa...

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Abstract

The invention discloses a negative pressure extraction and separation system and separation method for semi-volatile organic matter and non-volatile organic matter in samples. The present invention forms a continuous negative pressure and heating environment around the tested sample through the action of a vacuum pump and a heater. Under this environment, semi-volatile organic compounds and non-volatile organic compounds produce properties similar to volatile organic compounds, gasify to form steam and combine with the sample The matrix is ​​fully separated, and the separated organic matter vapor is transferred from the sample transfer pipeline to the adsorbent for adsorption and enrichment by the suction of the vacuum pump, and then the adsorbent containing the target compound is directly injected into the sample for analysis or thermal analysis, solvent desorption, and then enters the gas chromatography or gas chromatography / mass spectrometer for analysis. The extraction, purification and sample concentration of the present invention are completed simultaneously, greatly reducing the analysis cost and time.

Description

Technical field [0001] The invention relates to the technical field of sample pretreatment for chromatographic analysis, and specifically relates to a negative pressure extraction and separation system and a separation method for organic pollutants in a sample. Background technique [0002] According to the regulations of the World Health Organization WHO1989, (at room temperature) those with a boiling point from less than 0°C to 50°C are volatile organic compounds (VVOC), and those with a boiling point of 50°C-250°C are volatile organic compounds (VOC), which are saturated steam at room temperature The organic compound whose pressure exceeds 133.32Pa and the boiling point from 240-260℃ to 380-400℃ is called semi-volatile organic compound (SVOC), and the organic compound whose boiling point is higher than 380-400℃ is called non-volatile organic compound or granular organic compound ( POM). Organochlorine pesticides, organophosphorus pesticides, polycyclic aromatic hydrocarbons, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
CPCG01N30/06
Inventor 谢家理
Owner 谢家理
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